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International Journal of Green Energy, 3: 1–13, 2006
Copyright © Taylor & Francis Group, LLC
ISSN: 1543-5075 print / 1543-5083 online
DOI: 10.1080/01971520600704712

TREATMENT OF DICHLOROMETHANE USING

GLIDING ARC PLASMA

Antonius Indarto, Jae-Wook Choi, Hwaung Lee, and Hyung

Keun Song
Clean Technology Research Center, Korea Institute of Science & Technology

Decomposition of dichloromethane (CH2Cl 2) using a gliding plasma was examined 5

and reported in this paper. The effects of initial concentrations of CH2Cl2, total gas
flow rates, and input frequency have been studied to evaluate the performance of glid-
ing arc on CH2Cl2 decomposition. Using atmospheric pressure air as the carrier gas,
experimental results indicate that the maximum conversion of CH2Cl2 was 95.1% at a
total gas flow rate of 180 L/hr containing 1% by volume of CH2Cl 2. The reaction 10
occurred at an exothermic condition and gaseous products are dominated by CO,
CHCl 3, and Cl2. CO2 and CCl4 are also detected in the product stream in small
amounts. The conversion of CH2Cl 2 increases with the increasing applied voltage and
decreasing total gas flow rate.

Keywords: plasma; gliding arc; CH2Cl2 decomposition

15

INTRODUCTION 20
Nowadays, gaseous waste release to the atmosphere is growing in both amount and
complexity following the growth of industry and improvement of our living standards. Vari-
ous Chlorine-based compounds which are used in the widespread industrial sectors have a
high potential to emit some chlorinated volatile organics compounds (CVOC), such as
dichloromethane (CH2Cl2). The Environmental Protection Agency (EPA) Toxic Release
Inventory reports that U.S. industrial discharges of dichloromethane amounted to 29,000 25
metric tons in 1994 (Keene et al. 1999). This compound has an atmospheric half-life of sev-
eral months. Radical-chlorine atoms from CVOC will initiate and participate in ozone-
depleting reactions in the stratosphere (Sanhueza, 2001; US EPA, 1999; Khalil and Rasmus-
sen, 1999). It will create a big environmental problem when the compound is released with-
out any treatments (Shah and Singh, 1988). This situation shows that the rising of released 30
concentration of CVOC into the environment, together with its suspected toxicity and carci-
nogenic, has increased the demand for finding effective methods to reduce it.
The most widely adopted technique for the treatment of chlorinated VOC effluents
is thermal combustion or incineration (Lou and Chang, 1997). This method will process
influent of CVOC by direct oxidation reaction with air at a high temperature range, which 35
is between 800–1,100 °C. The main problem is relating to the incomplete combustion

Address correspondence to Antonius Indarto, Clean Technology Research Center, Korea Institute of Sci-
ence and Technology, P. O. Box 131, Cheongryang, Seoul 130-650, Korea. E-mail: indarto@korea.com.

1
2 A. INDARTO ET AL.

reaction. The reaction will produce numerous amounts of another complex chlorinated 40
compound (Taylor and Dellinger, 1988).
Catalytic oxidation is a well-known process for treating chloromethane. Unfortu-
nately, the most active catalyst for the oxidation usually comes from noble and expensive
metals, such as Platinum and Ruthenium, supported by alumina. High temperature process
is also required to increase the reaction rate and to overcome chloride poisoning (Alberici 45
and Jardim, 1997). Other limitation of plasma-assisted process is small flow rate of emis-
sion input process.
In recent years, many studies have been carried out on the application of new tech-
nologies to destruct the emission of CVOC. Plasma-assisted technology, such as RF
plasma (Lee et al., 1996), surface discharge reactors (Oda et al., 2002), dielectric barrier 50
discharge reactors (Tonkyn et al. 1996), pulsed discharge reactors (Yamamoto et al.,
1992), and capillary-tube type discharge reactors (Kohno et al., 1998), have been devel-
oped. Among non-thermal plasmas, gliding arc plasma has a good energy efficiency con-
version. This reason makes gliding arc plasma a bright prospect to be utilized for
industrial chemical reactions (Fridmann et al., 1999). In this study, gliding arc plasma was 55
used. It is an attractive method due to better production of radical species, higher flow
rates, and higher concentration of input material, to destruct dichloromethane (CH2Cl2).
However, destruction of chloromethane, carbon tetrachloride (CCl4) and chloroform
(CHCl3) in gliding arc plasma has been studied previously (Krawczyk and Ulejczyk
2003a; 2003b). The author reports that high destruction efficiency can be achieved using 60
this method.

EXPERIMENTAL SETUP
Input Gas
A schematic diagram of experimental setup is shown in Figure 1. Liquid CH2Cl2
which was used as the input material has a 99.0% purity (purchased from the Junsei 65
Chemical Co.). The carrier gas was atmospheric air and the flow rates were controlled
with a Mass Flow Controller (Tylan, FC-280S). The initial gas CH2Cl2 concentration was
set as 1, 2, 3, and 4% by volume. The flow rate of air to the plasma reactor was varied by
180, 240, and 300 L/hr.
Before entering the reactor, atmospheric air first passed through a scrubber and 70
mixed with CH2Cl2. Liquid CH2Cl2 was introduced by a syringe pump (KD Scientific,
Model 100) and a heater tape rolled covering the input line to vaporize the liquid CH2Cl2
into gas phase before it was mixed with air. The composition of the outlet stream was
analyzed before and after plasma operation.

Plasma Reactor and Applied Power System 75

The reactor was made from a quartz-glass tube of an inner diameter of 45 mm and a
length of 300 mm. Top and bottom of the reactor are equipped with teflon seals, the lower
comprising two electrodes made of stainless steel, the length of the electrodes being 150
mm. The distance of the electrodes in the narrowest section is only 1.5 mm. The gas mix-
ture is fed between the electrodes with a capillary of inner diameter 0.8 mm. A thermocou- 80
ple, located 10 cm above the electrode, is provided to measure the outlet gas temperature.
A high frequency AC power supply (Auto electric, A1831) is connected to the gliding arc
 TREATMENT OF DICHLOROMETHANE 3

vent to
atmosphere

FID GC TCD GC Mass

Column: Column: Spectro-
Benton Sieve meter
Carbon

MFC Plasma
Scrubber Reactor
Atmospheric
air

Heater tape
Syring pump

Figure 1 Schematic of experimental set up.

electrode to generate the plasma. Figure 2 shows the typical waveform of voltage and dis-
charge current used in these experiments.

Measurement System 85
The outlet gas composition is examined by an electron-impact ionization quadru-
pole mass spectrometer (Balzers, QMS 200) with software Quadstar 421. This software
is used for both qualitative and quantitative analysis of the inputs and products. Two
GCs are used to analyze the quantitative amount of products; CH2Cl2, also CHCl3 and
CCl4, in the gas mixture before and after the reaction are determined by GC-FID (Youn- 90
gLin M600D, Column: Bentone), for CO and CO2 by GC-TCD (YoungLin M600D,
Column: Carbon Sieve).
Chlorine gas (Cl2) is determined by bubbling the reaction gas through 0.05 M aque-
ous KI for a given time, followed by iodometric titration with 0.05 M Na2SO3 (Skoog
et al., 2000). 95
To evaluate the performance of system, selectivity and conversion, is used and
defined as:

moles of CH 2Cl2 consumed

Conversion of CH 2Cl2 = × 100%
moles of CH 2Cl2 introduced (1)

moles of CO formed
Selectivity of CO = × 100%
moles of CH 2Cl2 converted (2)
4 A. INDARTO ET AL.

6000

4000

2000
Voltage (V)

-2000

-4000

-6000

0.4 -2e-5 -1e-5 0 1e-5 2e-5

0.2
Current (A)

0.0

-0.2

-0.4

-0.6
-2e-5 -1e-5 0 1e-5 2e-5

Time (s)

Figure 2 Voltage and current profile of the applied electric power input.

moles of CO2 formed

Selectivity of CO2 = × 100%
moles of CH 2Cl2 converted (3)

moles of CHCl3 formed

Selectivity of CHCl3 = × 100%
moles of CH 2Cl2 converted (4)

moles of CCl4 formed

Selectivity of CCl4 = × 100%
moles of CH 2Cl2 converted (5)
 TREATMENT OF DICHLOROMETHANE 5

moles of Cl2 formed

Selectivity of Cl2 = × 100%
moles of CH 2Cl2 converted (6)

moles of CO formed + moles of CO2 formed + moles of CHCl3 formed

Carbon balance =
moles of CH 2Cl2 converted (7)

The supplied power was calculated as a product of voltage and current by oscilloscope
(Agilent 54641A). 100

RESULTS AND DISCUSSION

Effect of Concentration
CH2Cl2 was carried out at concentration range between 1% and 4% by volume and
diluted in atmospheric pressure air. In this study the experimental data was obtained 30
minutes after the initiation of the plasma of gliding arc, referred to as the stable tempera- 105
ture of the bulk gas as measured by thermocouple. Figure 3 shows the effect of CH2Cl2
initial concentrations variation on its conversion at a fixed power frequency of 20 kHz.
Conversion efficiency gradually decreases when the initial concentration of CH2Cl2
increases. The maximum conversion reaches 95.1% at 1% of CH2Cl2 concentration and
total air flow rate of 180 L/hr. Based on QMS spectra result (figure 8), the gaseous prod- 110
ucts are dominated by CO, CHCl3 and Cl2. Small amounts of CO2 and CCl4 are also

100

90

80
Conversion (%)

70

60

180 L/hr
50 240 L/hr
300 L/hr

40
0.5 1 1.5 2 2.5 3 3.5 4 4.5

CH2Cl2 concentration (%)

Figure 3 Effect of initial CH2Cl2 concentration on CH2Cl2 conversion (obtained at frequency of 20 kHz).
6 A. INDARTO ET AL.

Table 1 Effect of initial CH2Cl2 concentration on product selectivity.

concentration (% v/v) flowrate (L/hr) selectivity (%)

CO + CO2 CHCl3 CCl4 HCl Cl2

2 180 58.23 4.45 2.17 2.55 12.84

3 180 55.82 11.02 0.00 6.94 12.15
4 180 50.52 14.92 6.66 11.43 15.68
2 240 50.20 3.95 2.76 1.04 12.51
3 240 56.67 6.24 4.82 3.68 8.24
4 240 48.01 8.39 1.35 7.73 10.76

detected. CO2 is detectable when the initial concentration of CH2Cl2 is higher than 3%.
Compared to the yields of CO, the yields of CO2 was 4–7 times lower than CO yields in
the products. In this study, mass balance analysis of C (carbon) component is calculated
based on the total concentration of CO, CO2 and CHCl3. 115
Table 1 shows that more than half of reacted CH2Cl2 is converted into CO and CO2
as the products of the plasma reaction. High production of CO and CO2 reflects that oxy-
gen, which exists in the air at concentration of 20%, has a significant role in the decompo-
sition process. Less than 15% of reacted CH2Cl2 is transformed into other chloromethane
products, such as CHCl3 and CCl4. As shown in table 1, when the initial concentration of 120
CH2Cl2 is increased from 2% to 4%, the reaction selectivity of CO gradually decreases
from 58.2% to 50.5% at a total gas flow rate of 180 L/hr and 50.2% to 48% at 240 L/hr.
This result indicates that higher concentration of CH2Cl2 in the plasma reaction reduces
the possibility of product to form CO. However, at lower concentration of CH2Cl2, high-
active state oxygen e.g. O (3P and 1D) or O2 (a1Δ) enhances reaction with CH2Cl2 and 125
other chlorine-contained compounds rather than at higher concentration of CH2Cl2. In the
presence of atomic oxygen, CH2Cl2 can be removed by reaction (Fitzsimmons et al. 2000)

O + CH 2 Cl2 → CHCl2 + OH (8)

The production of OH in the system can help the destruction process by

OH + CH 2 Cl2 → CHCl2 + H 2 O (9)

CO is produced via oxidation of CH2Cl2 (Fitzsimmons et al., 2000; Hosson and Smith, 130
1999; Ho et al., 1992; Thuner et al., 1999; Bilde et al., 1999).

CH 2 Cl2 → CH 2 Cl + Cl (10)

CH 2 Cl2 + O2 → CH 2 ClO2 (11)

CH 2 ClO2 + CH 2 ClO2 → 2 CH 2 ClO + O2 (12)

CH 2 ClO2 + O2 → 2 HCOCl + HO2 (13)

 TREATMENT OF DICHLOROMETHANE 7

CH 2 ClO → HCOCl + H (14)

O, Cl + HCOCl → CO + ClO, Cl (15)

Other CO production pathways via secondary OH reaction and third body species are
also proposed (Lou and Chang, 1997; Fitzsimmons et al., 2000; Ho et al., 1992). 135

HCOCl + Cl → COCl + HCl (16)

OH + HCOCl → COCl + H 2 O (17)

COCl → Cl + CO (18)
A different phenomenon is found in chloroform (CHCl3) production. CH2Cl2 transfor-
mation into CHCl3 is higher when the initial concentration of CH2Cl2 is increased. Follow- 140
ing references (Hosson and Smith, 1999; Ho et al., 1992; Thuner et al., 1999; Bilde et al.,
1999), CHCl3 production is dependent on the presence and amount of Cl and CHCl2.

CHCl2 + Cl → CHCl3 (19)

Mostly, the source of Cl is obtained from unimolecular dissociation of CH2Cl2 145

CH 2 Cl2 → CH 2 Cl + Cl (20)

Increasing the initial CH2Cl2 concentration in the input stream will produce higher
amount of atomic Cl. Cl will easily collide with intermediate species CHCl2, produced by
reaction 8 and 9, to form stable gases such as CHCl3.
The ratio between total C (carbon) atom from gaseous products, e.g., CO, CO2,
CHCl3, CCl4 and total C atom from reacted CH2Cl2 has a range between 0.5 and 0.75. It 150
suggests that the major end products of plasma processing of CH2Cl2 diluted in atmo-
spheric air will be CO, CO2, CHCl3, and CCl4. The remaining C possibly goes to the solid
(shoot) or liquid production which is also produced during experiment.
However, in term of energy consumption, higher initial concentration of CH2Cl2
increases the energy consumption of plasma process, around 5–10 Watt for every 1% 155
increase in the concentration of CH2Cl2. Increasing amount of CH2Cl2 has a significant
effect on the alteration of voltage and current waveform which effects on power consump-
tion. In the presence of CH2Cl2 molecule, gliding plasma spends more energy to destruct
or break the chemical bond of CH2Cl2 to achieve a plasma state. Increasing concentration
of CH2Cl2 also has a significant influence on the increment of gas temperature. A stable 160
temperature is achieved after the gliding plasma system is on for 30 min. Compared with a
pure-air gliding arc, the gas temperature increases by 5–25 °C when the inlet stream con-
tains CH2Cl2. It shows that the destruction of CH2Cl2 is an exothermic reaction that
releases heat to the surrounding environment. The rising amount of destructed CH2Cl2
will produce more heat from the destruction reaction. 165
8 A. INDARTO ET AL.

Effect of Total Gas Flow Rate

The effect of total gas flow rate, which is related to the residence time of CH2Cl2 in
the reactor, was also examined. Figure 4 shows the CH2Cl2 conversion vs. total gas flow
rates at frequency of 20 kHz. The conversion of CH2Cl2 decreases when the total gas flow
rate is increased. Increasing total gas flow rate reduces the residence time of CH2Cl2 in the 170
reactor and hence the chance and time of CH2Cl2 to collide with electrons or other high-
energy state atoms or molecules.
Figure 5 clearly shows that the selectivity CO and CO2 decreases with the increasing
value of total gas flow rate. Following above explanation, increasing total gas flow rate
reduces the chance of collision reaction between CH2Cl2 and high-energy state species as 175
well as oxygen (atom or molecule). However, the carbon balance is also decreased with
increasing total gas flow rate.

Effect of Applied Frequency

Figure 6 shows the effect of various applied frequency of input power on the
CH2Cl2 destruction at 2% CH2Cl2 concentration and the total gas flow rate of 180 L/min. 180
The removal efficiency decreases from 90% to 55% when the applied frequency is
decreased from 20 kHz to 15 kHz. Decreasing applied frequency decreases the supplied
energy to the reactor, i.e., the energy used to dissociate the molecule of CH2Cl2. Figure 7
shows that reaction selectivity of CO relatively increased when the applied frequency was

100

90

80
Conversion (%)

70

60

1%

50 2%
3%
4%
40
150 170 190 210 230 250 270 290 310

Total Gas Flow Rate (L/hr)

Figure 4 Effect of total gas flow rate on CH2Cl2 conversion (obtained at the frequency of 20 kHz).
 TREATMENT OF DICHLOROMETHANE 9

CO and CO2 selectivity

60
Selectivity (%)

45

30

2%
3%
4%
15

0
Carbon balance

0.75
Carbon balance

0.60

0.45

2%
3%
0.30 4%

0.00
160 180 200 220 240 260 280 300 320

Total gas flow rate (L/hr)

Figure 5 Effect of total gas flow rate on CO2 and carbon balance.

also increased. On the other hand, the selectivity of CHCl3 is decreased. Increasing fre- 185
quency linearly correlates with increasing numbers of radical and high-active oxygen that
come out from atmospheric air, and tends to produce CO and CO2 as the gaseous end-
product. This is the possible reason why the selectivity of CO and CO2 increases with the
applied frequency.

QMS Spectra 190

QMS spectrum of the conversion of CH2Cl2 is shown in Figure 8. Figure 8 (top)
shows the peak components in the input stream. The baseline spectra of CH2Cl2 are m/z
83(CCl2+) and 85(CH2Cl2+) and this spectra was also owned by CHCl3. To distinguish
10 A. INDARTO ET AL.

100

80

60
Conversion (%)

40

20

0
14 15 16 17 18 19 20 21

Frequency (kHz)

Figure 6 Effect of applied input power frequency on CH2Cl2 conversion (obtained at the initial CH2Cl2 concen-
tration of 2% and the total gas flow rate of 180 L/hr).

between CH2Cl2 and CHCl3, we used a FID-GC as the analysis method. When the plasma
is on, as shown in Figure 8 (bottom), the peak intensity of m/z 83 and 85 are decreased and 195
some new peaks appear, e.g., m/z 61(COCl + ), 71(Cl2 + ), and 118(CHCl3 + ). It is evident
that COCl exists in the product stream because COCl has an important role in CO produc-
tion as an intermediate species.

CONCLUSION
The performance of CH2Cl2 conversion in gliding arc plasma at atmospheric pres- 200
sure was studied. Gliding plasma shows a good performance on the destruction of CH2Cl2
molecules. The maximum conversion of CH2Cl2 was 95.1% for feed gas stream contain-
ing 1% CH2Cl2 and air flow rate of 180 L/hr. The effect of the initial concentrations of
CH2Cl2, gas flow rates, and input power frequencies were also experimentally investi-
gated. Destruction of CH2Cl2 in gliding plasma environment occurred in an exothermic 205
 TREATMENT OF DICHLOROMETHANE 11

(CO+CO2) and CHCl3 selectivity 70

20

(CO+CO2) selectivity (%)

60
CHCl3 selectivity (%)

15 50

40
10
30

CHCl3 selectivity
5 (CO+CO2) selectivity 20

0 0
0.8
Carbon balance

0.6
Carbon balance

0.4

0.2

0.0
0 14 15 16 17 18 19 20 21
Frequency (kHz)

Figure 7 Effect of applied input power frequency on (CO + CO2) and CHCl3 selectivity and carbon balance.

reaction. CO, CO2, Cl2 and CHCl3 are the major product with a small amount of CCl4.
CO and CO2 selectivity achieved ~50% in all range of experimental condition. Transfor-
mation into other chloromethane compounds included a maximum of 15% for CHCl3
and 7% for CCl4. It is concluded that gliding arc plasma is adequate for CH2Cl2
reduction. 210

ACKNOWLEDGEMENTS
This study was supported by the National Research Laboratory Program of the Korea Minister of
Science and Technology.
12 A. INDARTO ET AL.

5e-10
before

4e-10

3e-10
Intensity

2e-10

1e-10

CH2Cl2, CHCl3

5e-10 after

4e-10
Intensity

3e-10

2e-10

1e-10
CO2

Cl2
CCl4
0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150

AMU (m/z)

Figure 8 QMS spectra of CH2Cl2 decomposition (obtained at the initial CH2Cl2 concentration of 2% and the
total gas flow rate of 180 L/hr).

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